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18162-48-6872-50-4Methylene ChloridenaphthaleneTHFTitanium Dioxide
ChemicalBook CAS DataBase List Tris (O-TBDMS)3
102522-47-4

Tris (O-TBDMS)3 synthesis

2synthesis methods
18162-48-6 Synthesis
tert-Butyldimethylsilyl chloride

18162-48-6
686 suppliers
$9.00/5g

77-86-1 Synthesis
Tris(hydroxymethyl)aminomethane

77-86-1
1052 suppliers
$5.00/25g

Tris (O-TBDMS)3

102522-47-4
28 suppliers
$160.00/1g

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Yield:102522-47-4 98%

Reaction Conditions:

with 1H-imidazole in N,N-dimethyl-formamide at 20; for 1 h;

Steps:

2.1.A

A) Synthesis of tris-(/ert-butyldimethylsilyloxymethyl)aminomethane, 2 Butyldimethylsilyl chloride (6.7g, 44.6mmol) and imidazole (6.3g, 92.9mmol) were dissolved in DMF (5mL). Tris(hydroxymethyl)methyl amine, 1 (1.5g, 12.4mmol) was added and the mixture stirred at room temperature for 1 hour. The product was washed with H2O, extracted with DCM, dried over anhydrous MgSO4 and filtered. Solvent was removed under reduced pressure to give a white powder (5.6g, 12.1mmol, 98%): 1H NMR (CDCl3) δ: 3.4 (s, 6H), 0.85 (s, 27H), 0.0 (s, 18H). 13C NMR (CDCl3) δ: 64.5, 57.1, 26.3, 17.9. LRMS (ES+) m/z 464.5 [100, (M+H+)].

References:

WO2009/50483,2009,A1 Location in patent:Page/Page column 26

18162-48-6 Synthesis
tert-Butyldimethylsilyl chloride

18162-48-6
686 suppliers
$9.00/5g

Tris (O-TBDMS)3

102522-47-4
28 suppliers
$160.00/1g

References